Fractionation or classification of finely divided solids



S. C. I YONS Nov. 7, 1939.

FRACTIONATION OR CLASSIFICATION OF FINEIY DIVIDEDASOLIDS Filed Feb. 2, 1938 CLHY CLHY LuRRY Patented Nov. 7, 1939 FRACTIONATION CR CLASSIFICATION F FINELY DIVIDED SOLIDS Sanford C. Lyons, Bennington, Vt., assignor to y Bird Machine Co., Walpole, Mass., a corporation of Massachusetts Application Februaryl, 1938, Serial No.1188,34`7

This invention relates to a process of fractionating or classifying finely divided solid materials of widely varying particle size into at least two fractions each of substantially uniform particle size or particle size range. It deals more especially with the fractionation of such finely divided solid materials containing a substantial fraction of particles of such iine size that they:

exhibit Brownian movement when suspended in water. and can hence be considered as being of colloidal neness.

In accordance with the present invention, aqueous suspensions of finely divided solid materials of widely varying particle size are subjected to an initial-stage eentrifuging treatment under conditions to deposit from suspension all but the very finest or colloidal particle fraction, Whereupon the centrifugally deposited fraction is resuspended in Water and the resulting aqueous suspension subjected to a second-stage gravitation-settling treatment, preferably in an upilow elutriator or its equivalent, under conditions to settle selectively the coarsest particles while the intermediate-sized particles and residual iinest or colloidal particles remain in suspension and are separated from the gravitationally settled coarsest particle fraction. Such a process is economical and advantageous in that each fractionating stage can be made to yield with high rate of output a solids fraction of substantially uniform particle size or particle size range.

In fractionating iinely divided solid material, it has sometimes beenlthe practice to suspend the material in water and to employ the differential settling properties of the variously sized particles in producing fractions of different particle size. A preferred specieY of fractionation known as elutriation involves progressively feeding a stream of the solids suspension into a tank near its bottom as suspension is progressively overowing the tank vand carrying with it only the relatively fine particles, since -the rate of feed of the suspension into the tank can be controlled so that the relatively coarse or heavy particles resist the momentum of the upflowing suspension and gravitate to the bottom of the tank. Fractionation of iinely'divided solid material by elutriation is, however, usually selective o`nly with relatively low solids content in the suspension; and in the case of nely divided solid material'containing a substantial fraction of very'ne or colloidal particles, seleetivityof fractionation is apt to be poor even with relatively low solids content in the suspension, unless a dispersing or deoccuating agent is added to the suspension for the (el. '20s- 12) purpose of peptizing or liberating the intlnsically very ne Aor colloidal particles. Otherwise, the very ne or colloidal particles tend to agglomerat or flocculate and to prevent, on account of socalled thixotropic effect, the differential settling of relatively coarse particles from the upowing suspension. Inrespect of the inherent thixotropy of colloidal fines, it might be noted that aqueous slurries or bentonite, which is of extraordinarily small average particle size, exhibit this property lil' to such a degree that slurries of a solids content of as low as 3%, even when they contain dispersing agent, are too viscous to allow the gravity subsidence therefrom of granular particles as course as '75 microns; and aqueous slurries of 40% solids l5 content exhibit a consistency reminiscent of mayonnaise.

The present invention thus utilizes a primary centrifugal-fractionating stage for segregating largely or practically completely the very ne or colloidal fraction from the original finely divided solid material and a secondary gravitationalfractionating or elutriating stage for fractionating or splitting the centrifugally deposited material into an intermediate-sized particle fraction and a coarsest particle fraction. The initial centrifugal-fractionating stage is eicient in segregating selectively the nest particle size fraction from the rest of the starting material even when the suspension of starting material being centrifuged is of high solids content, for the centrifuge is operated under conditions such that the natural differential settling properties of variously sized particlesis enormously multiplied. Because the aqueous suspension prepared from the centrifugally deposited solids of the centrifugal-fractionating stage is substantially devoid of very ne or colloidal particles, no trouble is had in realizing selectivity of fraction-y ation in a gravitational-fractionating or elutriating stage even when the aqueous solids suspension is run through such sta'gevatv comparatively high solids content and/or in the substantial absence of dispersing agent. It is thus possible to operate the secondary fraetionating or elutriating stage of the process hereof with high selectivity and high output, despite the fact that the equipment therefor is distinctly less expensive than that of the centrifuging stage.

While not limited thereto, the two-stage fractionating process is of especial utility as applied to crude clays', which generally contain particles v of widely varying sizes, namely, a fraction of very ne or colloidal particle size, a fraction of intermediate-sized particles, and a fraction of coarse particles, including such impurities as sand, mica, etc. Clays quarried in different geographical regions vary in their percentage or content of these fractions. For purpose of illustration, I shall deal herein specifically with the crude clays occurring at Dry Branch, Gordon, McIntyre, and other regions of central Georgia and generally containing about to 60% of clay particles ilner than about two microns, about 30% to 20% of intermediate-sized clay particles (i. e., particles ranging from about 2 to 45 microns), and about 20% of coarse particles, including roughly about 10% of oversized impurities of the nature of sand, mica, etc. Such clays may be economically fractionated by the process hereof into a relatively large clay fraction of very fine or colloidal particle size, which fraction is eminently satisfactory for use, for example, in paper-coating compositions, into a substantial clay fraction of intermediate particle size, which fraction is suitable for use, for example, as a filler for certain grades of paper and in the manufacture of ceramic ware, and into a fraction of relatively coarse particle size and containing lpractically all of the sand, micaI and other oversized impurities, which fraction is usually worthless and may be discarded.

With the foregoing and other features and objects in view, the present invention will now be described in further detail with particular reference to the accompanying drawing, which depicts schematically the more important apparatus for performing the two-stage fractionating process hereof.

Starting with crude clays such as have been indicated,` one may proceed to blunge the clay in water to produce a substantially homogeneous aqueous suspension or slip of, say, about 30% solids content. The lsuspension is preferably passed through a coarse screen which serves to remove therefrom floating trash, lumps of undisintegrated clay, etc., whereupon it is usually desirable to add to the screened suspension a small amount of dispersing or deiiocculating agent, such as sodium silicate, sodium phosphate, or the like. The addition of only about 0.2 to 1.0% of dispersing agent, based on the dry weight Aof the suspended solids, drastically reduces the viscosity of the suspension and conditions it for selective fractionation in a centrifuge at high solids content and with high rate of flow through the centrifuge.A The dispersed crude clay suspension having a solids content of about 30% may be delivered into a storage tank II for withdrawal and feeding at a substantially uniform rate into a centrifugal fractionator.

As illustrated, the aqueous clay suspension is withdrawn from the tank II by a pump I2 and delivered into a receiver I3 at such rate as to ensure therein a constant head or depth of suspension by constant overflow of suspension therefrom through a pipe I4 back to the tank II. The suspension thus kept at constant head in the tank I3 is fed at substantially uniform rate by way of a valved pipe I5 into a continuous-How centrifuge I0 near its open small-diameteror intake end. The centrifuge |10, which is preferably of the type disclosed in my Patent No. 2,085,538, dated June 29, 1937, is operated under substantially uniform solids-depositing condiloidal particles having a small-diameter end of 24". a largediameter end of 36", and a length of 50'? and haverotated such centrifuge at 900 R. P. M. as suspension oi' about 30% solids content containing about 0.4% sodium silicate, based on the dry .weight of the solids. was being fed thereinto at a rate of 65 gallons per minute. Under these conditions. the eiliuent from the centrifuge was an `aqueous suspension containing practically only the very fine or colloidal clay particles. Indeed, more than ot the solids suspended in the eilluent suspension were of average diameter less than 2 microns and such suspension was practically devoid of particles coarser than sixmicron average diameter. The solids fraction deposited on the centrifuge wall consisted essentially of particles coarser than two-micron aver-' age diameter and contained only al slight residuum of particles ner than two-micron average diameter.

The centrifugally deposited solids fraction is Y v shown as being progressively removed from the wall of the centrifuge by a helicoidal blade I6 and being discharged from the open small-diameter end of thecentrifuge into a trough Il, whereas the aqueous suspending vehicle or eiiluent containing suspended therein the finest or colloidal clay particles is shown as escaping from the centrifuge into a trough I8 through apertures 9 in the large-diameter end closure 8. The liquid eiliuent thus discharged from the centrifuge was found, under the particular conditions of operations hereinbefore described, to contain about 45% of the suspended crude clay fed into the centrifuge. Such eiliuent may be delivered from the trough I8 to any suitable system for the recovery of its ne or colloidal clay fraction. Thus, such liquid eiliuent may be treated with a suitable clay-nocculating agent, such as alum, and the fiocculated clay then recovered in filter presses or the like; or, if desired, the ine or colloidal clay fraction may be recovered -fromsuspension by passing such liquid eiiuent through an electrophoretic centrifuge of the type described in my Patent No.- 2,057,156, dated October 13, 1936, which type of centrifuge is designed especially for the purpose of causing subsidence or removal of extremely ne and colfrom suspension.

The centrifugally deposited solids as emitted under the conditions of operation hereinbefore described, through the open small-diameter end of the centrifuge into the trough I'I were found to be of stiff, pasty consistency and of a moisture content of about 40%. The solids `are shown as being progressively withdrawn from the trough I'I through a positive-feed sluice orconduit I9 to a mixing tank 20 equipped with agitators 2| and supplied with water from a valved pipe 22. Such solids may thus be resuspended in water in the tank 20 to produce a substantially uniform slurry or aqueous suspension, which maybe fed into an elutriating tank 23 by way of flow-regulating instrumentalities I2a, I3a, I 4a, and I5a similar to those in advance ofthe centrifuge I0. The lower or discharge end of the valved pipe I5a is shown near the tank bottom 2l, which is pref-v erably of shallow conical form and contains a central valved outlet pipe 25 through which the sludge or settled fraction of coarse solids may be withdrawn. The tank 23 may be cylindrical and be equipped near its top with an annular overflow gutter 26 leading to a. common overflow pipe 21.

As suspension is delivered into the elutriating tank 23 already filled with suspension to the an`` 75 nular overow gutter 26, the energy or frictional tractive force of viscous flow of the upowing suspension tends to carry with the suspension the nest particles, whereas the coarsest particles are suiiiciently heavy to resist the upiiowing currents.

tiallyonly particles of the desired intermediate size, say, particles finer than about 40 microns,

. which latter: size corresponds to about 325 mesh.

The clay fraction Vo f intermediate particle size present in the overflow suspension is useful for such purpose as illler in certain `grades of paper products.- The overow suspension may be treated in any suitable way for the recovery of its valuabley clay content. Thus, it may be delivered tosettling tanks,` wherein the clay particles may be allowed: to settle or concentrate to forma sludge of, say, about to 35% solids content, which sludge may be delivered to filter presses serving to remove practically completely the solids and to yield cakes of about 60l to '75% solids content. The cakes may be dried and shipped as lsuch or they may be pulverized as in hammermills, preparatory to shipment. The supernatent Water in the settling tanks may be decanted and reused for suspending fresh centrifugally deposited solids being fed from the centrifuge l0 to the mixing tank 20. The sediment or coarse particle fraction settling on the bottom of the tank 24 may beremoved progressively or intermittently through the valved discharge pipe 2 5 and discarded.

The suspension being fed progressively into the elutriating tank 23 may have a solids content upwards of about 10% and be practically devoid of dispersing agent, that is, contain no dispersing agent other than the minute residue of dispersing agent used .in 'preparing the-original dispersion of the crude or whole clay. In the case of ordinary crude clay containing a large or substantially fraction of colloidal or very ne particles, when a suspension of about 10% solids content is formed from the whole clayvin the substantial absence of dispersing agent, the resulting suspension. is'so viscous, on account Yof flocculation of colloidal particles or thixotropic effect, that particles of a diameter in the order of magnitude of 40 microns will not settle out differentially to the desired degree in an upilow elutriator at practical rates of flow through the Athat is, particles ner than about 2 microns,`

elutriator' Indeed, in such latter case, particles as coarse as, say, about 75 microns (200 mesh) are apt to remain suspended and enmeshed in the occulated or aggregated colloidal particles.

In the' case of the resuspended centrifugally deposited clay fraction delivered to the upow elutriator accordant with the process hereof, on the otherhand, the relative absence from the suspension of very ne and/ or colloidal particles,

makes `for a relatively fluent or low-viscosity suspension and, accordingly, makes possible aselective gravitational settling from the suspension of coarse particles even in the substantial absence of, dispersing agent and with substantial l solids lcontent in Ythe suspension and commercially satisfactory rates of flow of suspension through the upflow elutriator. In actual practice, it has been found possible by selective gravitational settling or elutriation accordant with the present invention to recover from the lsuspension of centrifugally deposited solids upwards of about Yof such solids in the form of a clay product composed practically completely of particles of less than about i5-micron average diameter and containingv but a very small percentage of. or practically no, particles finer than about Z-micron average diameter.

The rate of feed or upflow of the centrifugally V deposited solids suspension through the elutriator may vary considerably, for instance, between limits of about four feet per hour to about twelve feet per hour, depending upon such'factors as the largest size particles permissible in the overow suspension, the solids content of the suspension entering Vthe elutriator, Vthe temperature of the suspension, the depth of suspension in the elutriator, the shape of the suspended particles, etc. The temperature of the suspending water is mentioned as being an important factor, since, in the case of finely divided particles, even .a small change in viscosity `of the water brought about by change in thewater temperature is attended by appreciable change in the rate of sub-- sidence of the particles. Again, shape of the -suspended particles is animportant factor for the reason that particles of scaly or iiaky char acter are more resistant to settling thanparticles of round or jaggedA character. In other words, thev position of'equilibriumfor a subsiding particle is normal or penpendicular to its plane of greatest area; and sealy or flaky particles tend to assume'a position affording maximum resistance to subsidence through the suspending medium. While the presence or absence of dispersing agent Vin the suspension of centrifugally deposited fraction affects difierential settling of its variously sized particles,

such effect is not anywhere nearly as pronounced as in crude or whole clay suspension laden with the colloidal or very fine size clay particles. It is thus understandable why the desired selectivity of fractionation of the centrifugally deposited solids can be realized in the substantial absence of dispersing agent inthe\aqueo us suspension of such solids. VIt might`be noted that ,the particular conditions under which the ,gravitational-settling or elutriatingstages of the process hereof is to be performed, including the particular rate of ilow through such stage, can be empirically determined to yield voverflow sus-v pension containingsubstantially only the intermediate-sized particles, for instance, particles of about2 to 40 microns. A i

While itis possible to dispense withthe use of dispersing agent in the initial or .centrifugating stage of the process hereof, yet it is usually desirable to add a small percentage of dispersmg agent to the crude clay suspension so that such suspension may be vfractionated selectively at the desired high solids content in vthe.centrif ugating stage and vwith the desired high rate of suspension ow through this stage.` However, an important advantage of the process hereof is that it is possible to dispense entirely with the use of dispersing agent in fractionating by grav ity ...or elutriation the centrifugally deposited fraction andat the same time operate such gravity-fractionating or elutriating stage selectively ,and economically. 'In this connection, it must to sixty cents per-ton of clay. Moreover, clayproducing plants are frequently faced with the problem of being supplied with sufficient clean water for clay-processing. This is particularly 5 true of the clay regions in central Georgia, which are practically lacking in streams of clear water and whose rivers and brooks contain so much reddish or iron-oxide-contaminated clay and organic matter that it is necessary tofgo` to the trouble and expense of sinking wells and pumping well waterin tremendous volume to the clay-v producing plants. Because the volume of water used per ton of clay being processed is very large, it is customary'practice to reuse the water as many times as possible. However, when dispersing and occulatingagents are added to the clay-processing water, reuse of the Water cannot continue very long, since the water becomes contaminated by the water-soluble dispersing and occulating agents and theirv reaction products to such an extent that they are apt to re. tard or inhibit the eiiect of newly-added agents and also to contaminate unduly the nished clay product. 'Ihe factv is that when dispersing and/or occulating agents, which are generally Watersoluble electrolytes, are added to the clay-processing water and the water is reused excessively,

the concentration of water-soluble electrolytes in the water maybecome so great as to develop in the nished or dried clay cakes a crusty deposit that renders diicult resuspension of the clay in water to the desired ne particle size at its destination or place of use. Undue contamination of the iinished clay product with watersoluble electrolytes or salts is apt also to interfere with satisfactory use of the lclay in a paper mill, as by adversely aiecting such properties as retention of the clay by papermaking stock or by detracting from the desired printing and other properties inl papers coated with compositions containing the clay. 'Since at least the gravitational-fractionating or elutriating stage oi' the process hereof dispenses with the need of using dispersing and/or flocculating agent in the water of suspension passing through such stage, the processv hereof enables prolonged or o indennite reuse of such water in suspending the centrifugally deposited solids progressively emitted by the primary fractionating stage andat the same time yields an intermediate-sized clay fraction of the desired substantially complete freedom from water-soluble electrolytes or salts. The two-stage fractionatingprocess hereof may be applied advantageously to many nely divided solid materials other than crude clay and also to a solidfraction produced by other fractionating processes, especially when su'ch fraction contains, besides a main coarse particle component a material amount or residuum of w intermediate-sized particles and/or very line or colloidal particles and it is desired to separate` or recover such latter particles from the main coarse Vparticle component. For instance, Acalcined inorganic pigments, such as lithoponeand 65 titanium oxide, are usually ball-milled in water to form an aqueous slurry containing particles varying from colloidal particle size to palpable grit. Such ball-milled calcined pigment slurries may be subjected to the initial centrifugal-frac#` '70 tionating stage of the process hereof to produce a pigment fraction consisting practically entirely ot the very iinest or colloidal particles, say,

. particles ner than.about two-micron average diameter, which fraction is eminently suitable 75 for use in enamels and finishing paints of high aqueous suspension oi.' such material, which comopacity and light-reecting properties. The centrifugally deposited pigment fraction may be resuspended in water and subjected to the gravitational-i'ractionating or elutriating stage of the process hereofl to produce an intermediate-sized 5 particle fraction, say, one consisting practically entirely of pigment particles ranging from about two to about forty microns, which fraction is eminently suitable for use in so-called flat or base paints. The processing of such pigments 10 andthe recovery of the pigment fractions from suspension may be carried out much in the same way as hereinbefore described in connection with clay. As in the case of clay, itis desirable that the recovered pigment fractions be"practically 15 free from water-soluble salts or electrolytes; and no dispersing agent need be used Ain either the primary or secondary fractionating stage or at least in the secondary fractionating stage. The grit or coarsest pigment fraction represents y20 valuable material and may be returned to the ball mill for remilling in the presence of water along with freshly calcined pigment. The twostage fractionating process hereof may also be applied to such finely divided pigments, llers, 25 or other materials of widely varying particle size as zinc sulphide, zinc oxide, barium sulphate, calcium carbonate, etc., which materials may result from precipitation, fuming, sintering or calcination, or grinding naturally occurring mineral 30 or rock, such as calcium carbonate, orl articial mineral or rock, such as carborundum or other abrasive. i

I claim:

. 1. A process` of fractionating inely` divided 35 solid material of widely varying particle size, includingl a fraction of such fine particle size as tends to interfere materially with selective gravitational settling of coarser particles from an prises centrifuging an aqueous suspension of suchl material to deposit centrifugally substantially all but the very finest particle fraction, resuspendlng the centrifugally deposited fraction in water, and gravitationally settling from -the resulting suspension the coarsest particle fraction while maintaining above and removing from the gravitationally settled fraction an aqueous suspension of the intermediate-size particle fraction.

2. A process of fractionating nely divided solid material of widely varying particle size and including a fraction of relatively very fine or colloidal particle size tending to interfere materially with selective gravitational settling of coarser particles from an aqueous suspensionof such material, a fraction of intermediate particle size, and a fraction of relatively coarse particle size, which g comprises centrifuging an aqueous suspension of such material under conditions to deposit centrifugally substantially all but the very ne or .colloidal particle fraction, resuspending the centrifugally deposited fraction in water, and passing the resulting suspension through an upow elutriator under conditions of upfiow to settle gravitationally in the elutrlator thel coarsest particle fraction and thereby leave in the eiiluent suspension from the elutriator substantially only the intermediate-size particle fraction.

3. A process of fractionating 'finely divided solid material of widely varying particle size and including a fraction of relatively very ne orcolloidal particle size tending to interfere materially with selective gravitational settling of coarser particles from an aqueous suspension of such material, a fraction of intermediate particle size, and

, 2,179,154 a fraction of relatively coarse particle size, which` comprises centrifuging an aqueoussuspension of such material in -the `pres'ence ofa dispersing agent fo'r the very iine or colloidal particles and under conditons to deposit centriugallyl therefrom substantially all but the very ne or coldoidal particle fraction, resuspending the centrifugally deposited fraction in water practically free from dispersing agent, and passing theresulting suspension` through an upflow elutriator under conditions of upflow to settle gravitationally in the elutriator the coarsest particle fraction and thereby leave in the eliluent suspension from the elutriator substantially only the intermedil5 ate-size particle fraction.

4'. A process of fractionating substantially whole clay, which comprises centriiugillgY an aqueuos suspension of such clay to deposit centriugally substantially all but the very fine or colloidal particle fraction tending to interfere materially with selective gravitational settling Y of coarser particles from said aqueous suspension, resuspending the centriugally deposited fraction in water, and gravitationally settling from the resulting suspension of coarsest particle fraction, including the oversized impurities, while maintaining above and removing from the gravitationally settled fraction and aqueous suspenv sion of the intermediate-size particle fraction.

' 30 5. A process of fractionating .substantially whole clay, which comprises centrifuging an aqueous suspension of such clay under conditions to deposit centrifugally substantially all but the very fine or colloidal particle fraction tending to 35 interfere materially with selective gravitational settling of coarser particles from said aqueous suspension, resuspending the, centrifugally deposited fraction in water, and passing the resulting suspension through an upiiow elutriator 40 under conditions of upflow to settle gravitationally in the elutriator the coarsest particlefrac-V tion, including oversized impurities, and thereby leave in the emuent suspension fromtheelutriator substantiallyv only the intermediate-size particlefraction.

6. A process of fractionating substantially.

whole clay, which comprises centrifuging an aqueous suspension of such clay inthe presence of a dispersing agent for the very ne or colloidal particles and underconditions to deposit cen- .Y

triiugally substantially all but the very iine or colloidal particle fraction tending to interfere materially with selective gravitational Vsettling of coarser particles from said aqueous suspension resuspending the centrifngallyV v deposited fraction in water practically free 'from vdispersing agent, and passing the resulting suspension through an upilow elutriator under conditions of upow to-settle gravitationally in the elutri- .00 atar the coarsest particle fraction, including oversized impurities, and thereby leave inthe ellluent suspension from the elutriator substantialLv only theinte'rmediate-size particle fraction.

'7. A process of fractionating an aqueous calcined pigment suspension containing particles of widely varying particle size and including a fraction of relatively very ne or colloidal particle size tending to'interfere materially with I5- selective gravitational settling of coarser particles from said suspension, a fraction of intermediate particle size, and a fraction of relatively coarse particle size, which comprises centrifuging said suspension to deposit centrifugally substanl0 tially all but the very neor colloidal particle fraction, resuspending the centrifugally deposited fraction in Water, and gravitationallysettling and removing from the resulting suspension the coarsest particle ,fraction while maintaining 16 above and removing from the gravitationally settled fraction an aqueous suspension of the intermediate-size particle fraction.v

8. A process of fractionatin'g an aqueous calcined pigment suspension containing particles of- 20 Widely varying particle size and including a fraction of relatively very fine or colloidal particle size tending to interfere materially with selective gravitational settling of coarser particles from said suspension, arfraction'of intermediate par- 25 ticle size, and a fraction of relatively coarse particle size, which comprises centrifuging said suspension to deposit centrifugally substantially all but the very ne or colloidal particle fraction,

`resuspending the centrifugally deposited fraction in water, and passing the resulting suspension through an upilow elutriator under conditions of upilow to settle gravitationally in the elutriator lthe coarsest particlefraction and thereby leave in A.the very `inest or colloidal particle fraction and under conditions to deposit centrifugally substantially all but the veryv iine or colloidal particle 50 fraction, resuspending the centrifugally deposited `fraction in water pratically Afree from dispersing agent, and passingthe resulting suspension through an upflow elutriator under. conditions of upow vto settle gravitationally in the' elutriator 55 the coarsest particle fraction and thereby leavev in the efliuent suspension from the elutriator 'substantially only the intermediate-size particle fraction. i A Vv,

' SANFORD C.l LYONS. 00 

